PMID- 17723411 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20070829 LR - 20070828 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 571 IP - 1 DP - 2006 Jun 30 TI - Optimization of LC-MS/MS using triple quadrupole mass analyzer for the simultaneous analysis of carbosulfan and its main metabolites in oranges. PG - 1-11 AB - This paper describes an analytical method involving a simple solvent extraction for the simultaneous liquid chromatography coupled to quadrupole tandem mass spectrometry (LC-MS/MS) determination of carbosulfan, its most toxic metabolite--carbofuran--, and its other main metabolites--3-hydroxycarbofuran, 3-ketocarbofuran, 3-hydroxy-7-phenolcarbofuran, 3-keto-7-phenolcarbofuran, 7-phenolcarbofuran and dibutylamine--in oranges. Chromatography was performed on a Zorbax Bonus-RP (150 mm x 2.1 mm, 5 microm). The mobile phase was a ternary gradient water-methanol-acetonitrile with 1.0 mM ammonium acetate at flow rate of 0.2 ml min(-1). The LC separation and MS/MS optimization were studied to select the most appropriate operating conditions. The method developed has also been validated. The limits of quantification (LOQs) were from 1 microg kg(-1) for carbofuran to 10 microg kg(-1) for 3-keto-7-phenolcarbofuran. Extracts spiked with carbosulfan and its metabolites, at LOQ level, yielded average recoveries in the range 60-94%, with relative standard deviations (R.S.D.s) less than 15%. Calibration curves for carbosulfan and its metabolites (range LOQ-1000LOQ) were linear, with coefficients of correlations better than 0.990. The method was successfully applied to establish the primary degradation products in oranges treated with carbosulfan. The LC-MS/MS method developed is simple, rapid, and suitable for the quantification and confirmation of carbosulfan and seven of its main metabolites in orange at levels lower than 10 microg kg(-1). FAU - Soler, Carla AU - Soler C AD - Laboratori de Bromatologia i Toxicologia, Facultat de Farmacia, Universitat de Valencia, Av. Vicent Andres Estelles s/n, 46100 Burjassot, Valencia, Spain. carla.soler@uv.es FAU - Hamilton, Brett AU - Hamilton B FAU - Furey, Ambrose AU - Furey A FAU - James, Kevin J AU - James KJ FAU - Manes, Jordi AU - Manes J FAU - Pico, Yolanda AU - Pico Y LA - eng PT - Journal Article DEP - 20060427 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 EDAT- 2007/08/29 09:00 MHDA- 2007/08/29 09:01 CRDT- 2007/08/29 09:00 PHST- 2006/03/18 00:00 [received] PHST- 2006/04/11 00:00 [revised] PHST- 2006/04/13 00:00 [accepted] PHST- 2007/08/29 09:00 [pubmed] PHST- 2007/08/29 09:01 [medline] PHST- 2007/08/29 09:00 [entrez] AID - S0003-2670(06)00868-3 [pii] AID - 10.1016/j.aca.2006.04.033 [doi] PST - ppublish SO - Anal Chim Acta. 2006 Jun 30;571(1):1-11. doi: 10.1016/j.aca.2006.04.033. Epub 2006 Apr 27.